CN105092569B - The measuring method of calcium hydroxide content in carbide slag - Google Patents
The measuring method of calcium hydroxide content in carbide slag Download PDFInfo
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- CN105092569B CN105092569B CN201510516325.XA CN201510516325A CN105092569B CN 105092569 B CN105092569 B CN 105092569B CN 201510516325 A CN201510516325 A CN 201510516325A CN 105092569 B CN105092569 B CN 105092569B
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Abstract
The invention discloses a kind of measuring methods of calcium hydroxide content in carbide slag, it is short the purpose is to provide a kind of operating process, it is at low cost, quickly, efficiently, accurately, stability is good, the method of calcium hydroxide content in the measurement carbide slag for being easy to grasp, one is added the calcium carbide slag sample that quality is m in beaker, another is not added as blank control, it is separately added into hydrochloric acid dissolved samples on low temperature electric hot plate later, after sample dissolution, it removes, after cooling, successively add triethanolamine respectively, water, hydroxylamine hydrochloride, later plus potassium hydroxide solution, add a few drop magnesium sulfate, calcein indicator is appropriate, it is terminal that the EDTA standard solution for being C with concentration, which is titrated to fluorescence green disappearance, several lower volumes are respectively V and V0, obtained calcium hydroxide content are as follows: WCa(OH)2%=C (V-V0)MCa(OH)2100/m×100。
Description
Technical field
The present invention relates to slag analysis technical fields, and in particular to calcium hydroxide content in a kind of volumetric determination carbide slag
Measuring method.
Background technique
Carbide slag, calcium carbide hydrolysis generate after obtaining acetylene gas with calcium hydroxide waste residue as main component, domestic carbide
Production acetylene necessarily produces ancillary industry waste carbide slag (paddle), acetylene (C2H2) it is one of important source material of basic organic synthesis,
Using calcium carbide as raw material, adds the simple process of water (wet process) production acetylene mature, account for larger specific gravity in China at present.1t calcium carbide adds water
More than 300 kg acetylene gas are produced, while generating the industrial stoste of 10t solid content about 12%, are commonly called as carbide slag slurries.Utilize calcium carbide
Slag can replace lime cement made of stones, carbide raw material is used as instead of lime stone, production chemical plant product, produce construction material and be used for
Environmental improvement etc..It is mainly stored and acts on as follows: 1, filling out sea, fills out the regular stacking of ditch；2, it is sold after natural subsidence；3, it produces
Lime stone is as carbide raw material；4, light-weight brick is produced；5, calcium carbide waste slag is used as industrial chemicals；6, carbide slag is mainly for the production of building
Build material；7, there are also some other purposes, such as brickmaking, cement processed, mortar processed and hemp-fibred plaster, bleaching liquid processed.
Carbide slag (paddle) mainly has two digestion approach at present.First is that using dry slag is formed as cement after the dehydration of carbide slag paddle
The raw materials for production of equal building materials；Second is that making calcium carbonate is substituted as the desulfurizing agent of power plant desulphurization system after carbide slag paddle filtration, purification
With.In smelter generally as desulfurizing agent.
Carbide slag main component is calcium hydroxide, however hydroxide calcium catalyst does not have the measurement of standard in carbide slag at present
Method, therefore the Accurate Determining for carrying out calcium hydroxide in carbide slag is of great significance.
Summary of the invention
It is at low cost the technical problem to be solved in the present invention is to provide a kind of operating process is short, quickly, efficiently, it is accurate, stablize
Property it is good, be easy to grasp measurement carbide slag in calcium hydroxide content method, solve carbide slag in calcium hydroxide content measurement
The problem of without standard determination method.
In order to achieve the above object, in a kind of carbide slag of the present invention calcium hydroxide content measuring method, comprising the following steps:
One is added the calcium carbide slag sample that quality is m in beaker, another is not added as blank control, adds respectively later
Enter hydrochloric acid dissolved samples on low temperature electric hot plate to remove after sample dissolution, after cooling, successively adds triethanolamine, water, salt respectively
Sour azanol, later plus potassium hydroxide solution, plus a few drop magnesium sulfate, calcein indicator is appropriate, the EDTA standard for being C with concentration
It is terminal that solution, which is titrated to fluorescence green and disappears, and writing down volume is respectively V and V0, obtained calcium hydroxide content are as follows: WCa(OH)2%=
C(V-V0)MCa(OH)2100/ m×100；
In formula: MCa(OH)2: the molal weight of calcium hydroxide, g/mol；
M: sample mass, g；
C:EDTA concentration of standard solution, mol/L；
V: sample consumes the volume of EDTA standard solution, mL；
V0: blank consumes the volume of EDTA standard solution, mL.
Wherein the concentration of hydrochloric acid is 25%.
Wherein the temperature of dissolved samples is 100 DEG C on the Low-temp. electrothermal plate.
Wherein the triethanolamine concentrations are 12%.
Wherein the potassium hydroxide solution concentration is 20%.
Wherein the Adlerika concentration is 0.5%.
The invention difference from existing technology is that the present invention achieves following technical effect:
1, this method directly shelters interference element with triethanolamine in titration, without precipitating after sample dissolution
It separates, be filtered, washed.Analysis time is substantially reduced, reduces loss, improves accuracy.Production efficiency is improved, is reduced
Reagent consumption and cost of labor；
2, the present invention has formulated the measuring method of calcium hydroxide content in carbide slag, can be used for producing detection, Instructing manufacture
Technique；
3, the method for the present invention is stable, accurate, and operating process is short, at low cost, quickly, efficiently, is easy to grasp.
Specific embodiment
With reference to embodiments, the forgoing and additional technical features and advantages are described in more detail.
1. method summary: using hydrochloric acid (25%) dissolved samples in 300mL beaker, remove, after cooling, add tri- second of 50mL
Hydramine (12%) (has to first addition, be to first shelter the interference elements such as iron and aluminium), adds 50mL water, adds hydrochloric acid
Azanol is a little, and (further masking action) adds 30mL potassium hydroxide solution (20%), and (effect of buffer solution) adds a few drop sulphur
Sour magnesium (0.5%) (keeping terminal good-looking), appropriate calcein, being titrated to fluorescence green disappearance with EDTA standard solution is terminal.
2. reagent:
2.1 hydrochloric acid (25%)
2.2 hydroxylamine hydrochlorides (solid)
2.3 triethanolamines (12%)
2.4 potassium hydroxide solutions (20%)
2.5 calcein indicator: the finely ground mixing of sodium chloride after 1g calcein and 100g drying is placed in port grinding bottle
It is spare.
2.6EDTA standard solution C (EDTA)=0.01783mol/L
2.7 magnesium sulfate (0.5%)
3. sampling and sample preparation: taking sample preparation standard to carry out sample according to slag and produce.
4. sample weighting amount: weighing sample 0.0500g
5. analytical procedure:
Sample 0.0500g is weighed in 300mL beaker, 20mL hydrochloric acid (25%) is added on low temperature electric hot plate (100 DEG C)
Dissolved samples are removed after sample dissolution, after cooling, add 50mL triethanolamine (12%) (have to first addition, be in order to
The interference elements such as iron and aluminium are sheltered first), add 50mL water, add hydroxylamine hydrochloride a little, (further masking action) adds 30mL hydrogen
Potassium oxide solution (20%), (effect of buffer solution) adds a few drop magnesium sulfate (0.5%) (keeping terminal good-looking), and calcein is suitable
Amount, being titrated to fluorescence green disappearance with EDTA standard solution is terminal.Writing down volume is V.
Blank:
In 300mL beaker, it is molten that 20mL hydrochloric acid (25%) dissolved samples, sample on low temperature electric hot plate (100 DEG C) is added
Xie Hou is removed, and after cooling, added 50mL triethanolamine (12%), is added 50mL water, add hydroxylamine hydrochloride a little, add 30mL potassium hydroxide
Solution (20%) adds a few drop magnesium sulfate (0.5%), and appropriate calcein, being titrated to fluorescence green disappearance with EDTA standard solution is
Terminal, writing down volume is V0。
6. Analysis result calculation:
WCa(OH)2%=C (V-V0)MCa(OH)2100/m×100
In formula: MCa(OH)2: the molal weight (g/mol) of calcium hydroxide
M: sample mass (g)
C:EDTA concentration of standard solution (mol/L)
V: the volume (mL) of sample consumption EDTA standard solution
V0: the volume (mL) of blank consumption EDTA standard solution
7. sample analysis compare: due in carbide slag hydroxide calcium catalyst without suitable standard specimen
Precision test data such as table 1:
The calcium hydroxide content value repeatedly measured in 1 carbide slag sample of table
| The name of an article | Measured value (%) |
| Carbide slag 1 | 81.63 81.60 81.59 81.62 81.65 |
| Carbide slag 2 | 85.46 85.47 85.50 85.51 85.45 |
| Carbide slag 3 | 84.53 84.56 84.60 84.63 84.70 |
| Carbide slag 4 | 82.69 82.70 82.75 82.60 82.63 |
As can be seen from Table 1: measurement result precision is good.
8. conclusion:
The content of calcium hydroxide in carbide slag can be accurately determined by the method for the invention.When substantially reducing operation
Between, reduce energy consumption.So that determination data is accurate and reliable, application obtains preferable effect in production.
Embodiment described above only describe the preferred embodiments of the invention, not to model of the invention
It encloses and is defined, without departing from the spirit of the design of the present invention, those of ordinary skill in the art are to technical side of the invention
The various changes and improvements that case is made should all be fallen into the protection scope that claims of the present invention determines.
Claims (1)
1. the measuring method of calcium hydroxide content in a kind of carbide slag, it is characterised in that the following steps are included:
One is added the calcium carbide slag sample that quality is m in beaker, another is not added as blank control, is separately added into salt later
Acid dissolved samples on low temperature electric hot plate are removed after sample dissolution, after cooling, successively add triethanolamine, water, hydrochloric acid hydroxyl respectively
Amine, later plus potassium hydroxide solution, plus a few drop magnesium sulfate, calcein indicator is appropriate, the EDTA standard solution for being C with concentration
Being titrated to fluorescence green and disappearing is terminal, and writing down volume is respectively V and V0, obtained calcium hydroxide content are as follows: WCa(OH)2%=C
(V-V0)MCa(OH)2100/m×100；
In formula: MCa(OH)2: the molal weight of calcium hydroxide, g/mol；
M: sample mass, g；
C:EDTA concentration of standard solution, mol/L；
V: sample consumes the volume of EDTA standard solution, mL；
V0: blank consumes the volume of EDTA standard solution, mL；
The concentration of hydrochloric acid is 25%；
The temperature of dissolved samples is 100 DEG C on the low temperature electric hot plate；
The triethanolamine concentrations are 12%；
The potassium hydroxide solution concentration is 20%；
The Adlerika concentration is 0.5%.
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| CN105758852A (en) * | 2016-02-26 | 2016-07-13 | 内蒙古包钢钢联股份有限公司 | Determining method for content of calcium in high-calcium line |
| CN105651930A (en) * | 2016-02-26 | 2016-06-08 | 内蒙古包钢钢联股份有限公司 | Method for determining calcium content of iron-calcium cored wire |
| CN108507899B (en) * | 2018-04-04 | 2021-03-09 | 青海盐湖工业股份有限公司 | Electrolytic metal magnesium bath slag analysis method |
| CN111398091A (en) * | 2020-03-05 | 2020-07-10 | 柳州钢铁股份有限公司 | Analysis method for determining calcium carbide in composite silicon carbide deoxidizer for steelmaking |
| CN112229977B (en) * | 2020-09-03 | 2023-03-17 | 神华国能集团有限公司 | Method for determining proportion of carbide slag in coal as fired |
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| CN104458731A (en) * | 2014-12-10 | 2015-03-25 | 内蒙古包钢钢联股份有限公司 | Method for joint measurement of calcium-barium content of silicon-barium alloy by using compleximetry |
| CN104483311A (en) * | 2014-12-10 | 2015-04-01 | 内蒙古包钢钢联股份有限公司 | Indicator for simultaneous measurement of calcium, barium and magnesium in silicon-calcium-barium-magnesium by adopting EDTA titration method |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN104458731A (en) * | 2014-12-10 | 2015-03-25 | 内蒙古包钢钢联股份有限公司 | Method for joint measurement of calcium-barium content of silicon-barium alloy by using compleximetry |
| CN104483311A (en) * | 2014-12-10 | 2015-04-01 | 内蒙古包钢钢联股份有限公司 | Indicator for simultaneous measurement of calcium, barium and magnesium in silicon-calcium-barium-magnesium by adopting EDTA titration method |
Non-Patent Citations (1)
| Title |
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| 电石渣中氢氧化钙测定方法的改进;吕文涛;《科技致富向导》;20121231(第17期);第266页 |
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